新疆红枣中环磷酸腺苷含量的LC-MS/MS法测定研究

Determination for Cyclic Adenodsine Monophosphat in Xinjiang Zizyphus jujube by LC-MS/MS

建立了LC-MS/MS法来测定红枣中环磷酸腺苷(cAMP)的含量,采用ZORBAX SB-Aq C18色谱柱(3.5μm,4.6 mm×150 mm),柱温为30℃,以水-乙腈(40︰60)为流动相,流速为0.6 mL/min,被测成分cAMP的监测反应质荷比分别为m/z 330.10～136.00。cAMP在0.50～1 000μg/L质量浓度范围内呈良好线性,相关系数大于0.999 0,检出限为0.10μg/kg。3个浓度梯度(1.00, 50.0和500.0μg/kg)的平均回收率在91%～106%之间,相对标准偏差(RSD, n=6)在1.5%～12.7%之间。该方法灵敏度高、定性定量准确、重现性好、专属性强,适用于红枣中环磷酸腺苷的检测。

To establish a method for the determination of cyclic adenodsine monophosphat （cAMP） in Zizyphus jujube by liquid chromatography-tandem mass spectrometry （LC-MS/MS）, the chromatographic analysis was carried out by ZORBAX SB-Aq C18 column （3.5 μm, 4.6 min×150 mm） and the column temperature was 30℃. The mobile phase consisted of water-acetonitrile （40 ： 60） at a flow rate 0.6 mL/min. Detection and quantification were performed by mass spectrometry in multiple reaction monitoring mode with m/z 330.10-136.00 for cAMP. cAMP had good linear correlations in the range of 0.50-1 000 μg/L, with all correlation coefficients above 0.999 0. The detection limits of cAMP were 0.10 Ixg/kg. The average recoveries of there con-centrations （1.00, 50.0 and 500.0 μg/kg） were between 91% and 106%, and the relative standard deviations （RSD, n=6） were between 1.5% and 12.7%. This method was highly sensitive, accurate, reproducible and proprietary. It was suitable for the detection of PAEs in Ziziphus iuiube.